反应 #674372
ord-33114cb8a6f441e78678e62c62157006
反应方程式
Ethyl 4-formyl-2-methylbenzoate
4-formyl-2-methylbenzoic acid
H2SO4
→
title compound
收率 80.0%
Ethyl 2-methyl-4-vinylbenzoate
收率 80.0%
溶剂
反应条件
温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度The reaction mixture was cooled to 25° C.
- 2浓缩concentrated under reduced pressure
- 3workup.ADDITIONThe residue was diluted with EtOAc
- 4洗涤washed with water
- 5洗涤The combined EtOAc extracts were washed with brine
- 6干燥dried over Na2SO4
- 7浓缩concentrated under reduced pressure
实验过程
Ethyl 4-formyl-2-methylbenzoate (AI16). To a stirred solution of 4-formyl-2-methylbenzoic acid (3 g, 18.2 mmol) in EtOH (30 mL) was added conc. H2SO4 (2 mL) and the reaction mixture was heated at 80° C. for 18 h. The reaction mixture was cooled to 25° C. and concentrated under reduced pressure. The residue was diluted with EtOAc and washed with water. The combined EtOAc extracts were washed with brine, dried over Na2SO4 and concentrated under reduced pressure to afford the title compound as a solid (2.8 g, 80%): 1H NMR (400 MHz, CDCl3) δ 10.05 (s, 1H), 8.04 (m, 1H), 7.75 (m, 2H), 4.43 (m, 2H), 2.65 (s, 3H), 1.42 (m, 3H).